Disperse system and process of making same



Patented a... 27, 1933 UNITED- STATES PATENT oFFicE ms KKGI, or BASEL,SWITZERLAND, Assrouon 'ro SOCIETY or CHEMICAL INDUSTRY 11v BALE, orBASEL, swrrznnrann msrnnsn SYSTEM AND rnocrss or manure sum 80 Drawing.

The present invention relates to the manufacture of disperse systems. Itcomprises the process of making these systems, the disperse systemsthemselves as .well as the application of these systems for theimprovement of textiles, and the textiles improved with aid of thesesystems. a

It is known that forthe manufacture of disperse systems the salts ofpartially acylated polyamines are used with advantage as emulsifyingagents, it being indifferent Whether the non-acylated amino groups ofthe polyamine are present in the form of a primary, secondary ortertiary base or in the form of a quaternary ammonium compound. Suchpartially acylated polyamines are inter alia disclosed in the U. S.Patents 1,534,525 and 1,737,458. Other partially acylated polyamines arefor example such which derive from diamines containing OH- oups, forexample the oleyl-B-hydroxyiethylamino propyl amide and the ammoniumcompounds thereof, as also such which derive from cyclic diamines,para-amino-dimethyl-aniline and the ammonium compounds deriving.therefrom, such as the addition product of dimthyl-sulfate to the abovecompound, the 4-oleylamino- (diethyl-amino-ethyl methyl) -aniline of theformula these products those are particularly valuable which derive fromhigh molecular acids.

among these there maybe mentioned palmi-.

such as the stearyl tinic acid, stearicacid and oleic acid, lauric acid,the naphthenic acids, abietic acid, and the like.

If with the aid of these compounds lipoidsoluble substances, such asoils, fats, waxes, hydrocarbons (solid or liquid, particularly of highermolecular weight with more than 14 carbon atoms), terpenes, andthe'like, are to be emulsified with water, the success is not alwayssatisfactor The surprising observation has now been made thatessentially better results are obtained if the emulsification of thesaid substances with solutions of the salts of partially acylatedpolyamines is carried out in presence of at least one further protectivecolloid. Such protective colloids are, soaps, gall acids and theirderivatives, sulfonic acids of high molecular acids and their salts,sulfite cellulose waste liquors, lurkey red oil, albumin, gelatin, glue,saponin, natural and artificialresins, derivatives of cholesterine,phosfatides, gelloses, gum, natural and artificial waxes, wool waxes, solvents and softening agents, organio bases and their salts, inorganiccolloids, and the like. In the case of oils, fats and Waxes whichcontain free fatty acids, the "production of the further protectivecolloid may be carried out with addition of small quantities of anorganic or inorganic base, so thatformation of a water-soluble soaptakes place, which plays the part of the protective colloid. Theaqueoussolutions thus produced, which are characterized by the presenceof a lipoidsoluble substance, of a salt of a partially acylatedpolyamine, tective colloid, are of a great technical importance for avarietyof purposes. They are particularly very valuable in the textlleindustry for Water-proofin textiles, the production of sizings and soteners, etc.

The following examples describe the production of such emulsions.

Example 1 Applicationv filed larch 14, 1931, Serial No. 522,778, and'inSwitzerland March 22,1980.

for example,

and of a further pro- I strength. In this then 1000 parts of olive oil,while stirring vigorously. There is obtained a stable, milky emulsion.

E mample 2 of a sodium oleate solution of per cent.

strength and agitation there is obtained a fine, highly dispersedemulsion.

- Example 3 20 parts of the sulfate of the conversion product quantityof unsymmetrical, diethyl-ethylenediamine, calculated on thesaponification number, are dissolved in 1000 parts of water. Afteraddition of 60 parts of a solution of 10 per cent. strength of an alkalisalt of the di-isopropyl-naphthalene-sulfonic acid, the whole isvigorously shaken with 500 parts of chloro-benzene. An emulsion is thusobtained which is considerably finer and more stable than the emulsionwhich has been made with a 2 per cent. solution of the above sulfate, ora 2'per cent. solution of the salt of thedi-isopropyl-naphthalene-sulfonic acid alone.

Ewample 4 Petroleum, in which 4 per cent. of lanolin have beendissolved, is emulsified with an aqueous solution of 5 per cent.strength of the oleyl-diethyl-ethylene-diamine hydrochloride. Anemulsion is thus obtained which is very much finer and more stable thanwithout addition of lanolin.

Example 5' Ewample 6 450 parts of paraffin oil, 50 parts of lanolin and20 parts of oleyl-aminoethyl-diethyl-benzyl-ammonium chloride are heatedAt about 7 5 C. there are run in,

together. while stirring well, 480 parts of sodium oleate solutioncontaining 28.2 parts of oleic acid and 4 parts of sodium hydroxide.After cooling, a thick colloidal solution of paraffin oil is obtainedwhich can be freely diluted with water.

Ewample 7 200 parts of turpentine oil and 100 parts of a solution ofoleylamino-ethyl-diethylof castor oil with the theoretical.

methyl-ammonium-methylsulfonate of 10 per cent. strength, are mixedtogether and, while agitating vigorously, there are added in doses 28parts of 0.5 N-solution of sodium abietinate. There .is thus obtained acolloidal solution of turpentine.

E wample 8 1000 parts of a solution ofoleylaminoethyl-diethyl-methyl-ammonium methylsulfonate of 10 per cent.strength are diluted with 500 parts of water in which are dissolved 3.2parts of sodium hydrovide. 1500 parts of boiled linseed oil are addedand by shaking there is obtained a stable, finely dispersed linseed oilemulsion.

Ewample 9 900 parts of parafiin wax are melted and 100 parts of beeswaxand 40 parts of ole amino-ethyl-diethyl-benzyl-ammonium-ch o ride arestirred into the'fused mass. To this mixture, heated at a temperatureabove the melting point of the paraflin there is run in,

while stirring well, a solution of 95 parts of Ewample 10 Cotton satinis impregnated as follows The material is padded in a solution of 2kilos of the emulsion prepared according to the particulars given in thefirst paragraph of Example 9 in 100 parts of water of ordinarytemperature, dried on a stretching frame, moistened and calendered underpressure. The material thus finished is characterized by its beautifullustre.

Example 11 A solution is prepared from 9 kilos soluble starch, 5 kilosglucose sirup, 3 kilos of the emulsion prepared according to theparticulars of the 1st paragraph of Example 9, and 1 kilo of soap in 100litres water. This finish serves for the finishing of canvas formattresses which is then distinguished by a solid linen-like feel. Inthis example as well as in the preceding example, the emulsion of thefirst paragraph of Example 9 may partly be replaced by the emulsionsmentioned in the second paragraph of Example 9.

. Artificial silk islfinished .8 follows 3 kilosofthe'emulsion. preparedaccording to the particulars of Example 1 are added to .100 litres ofwater and the material is unpregnat'ed with. this solution once ortwice,

. whereupon it ishydro-extracted and dried.

The

f artificial silk is distinguished by a fine eel.

Example 13 Rain coat "cloth is waterproofed by impregnation with thefollowing solution in the single-bath process I 100 parts of water aremixed with a solu- 4 tion of 200 rams Marseilles soa to which with goodstlrring 500 grams of t e emulsion obtained according to the particularsof the first paragraph of Example 9 are added. 3 litres of acetate ofalumina of 6 B6. are then added, while vigorously stirring, whereuponthe impregnation operation is commenced.

This latter operation is preferably conducted 'on the padding machine,and the goods,

without washing, are then subjected to the drying rocess. The ciualityof being waterproo of the materia impregnated in this manner is betterthan in the case of the material treated according to the usual twobathprocess with soap and, acetate of alumina.

E'wample 14 For the sizing of artificial. silk 400 grams of potatmstarchare made into a' paste with litres of water, to which 50 litres coldwater and 300 grams of the emulsion prepared according to theparticulars of the first para-- graph of Example 9 are added. Thematerial is impregnated as usual with the sizing mass,hydro-extractedand dried. The artificial silk sized in this manner isdistinguished'by its smooth surface which is of great advantage for itssubsequent workingup in the weaving or knitting mills.

What I claim is 1. A process for the production of dis-' perse systemsfrom lipoid-soluble substances ,7

and water, consisting in emulsifying lipoidsoluble substances with aidof salts of .partially acylated polyamines, in presence of soaps andwaxes as protectivecolloids, with water. f v 2. A process for theproduction of disperse systems from lipoid-soluble substances and water,consisting. in emulsifying lipoidsoluble. substances ,with aid of saltsof systems from lipoid-soluble substances and polyamines partiallyacylated with high molecular acids, in presence of soaps and waxes asprotective colloids, with water.

3. A process for the production of disperse water, consisting inemulsifing lipoid-soluble substances with aid of sa ts of polyamines partiallyacylated with high molecular fatty acids, in

-ble substances with aid of salts of plresenceofsoaps and waxes asprotective co oids, with water.

.4. A process for the production of disperse systems from lipoid-solublesubstances and water consisting in emulsifying lipoid-soluble substanceswith aid of salts of aliphatic diamines partially acylated with highmolecular fatty acids, in presence of soaps and waxes as protectivecolloids, with water.

5. .A process for the roduction of dis perse systems froin lipoi-s01ub-le substances and water, consisting in emulsifying lipoidsolublesubstances with aid of salts of unsymmetricall alkylated diaminespartially acylated wit high molecular fatty acids containing 15 to 17carbon atoms, in presence of soaps and waxes as protective colloids,with water.

6. A process for the production of disperse systems from lipoid-solublesubstances and water, consisting in emulsifying lipoid-soluunsymmetricaldiethylethylenediamine partially,

acylated with high molecular fatty acids contaming 15 to 17 carbonatoms, in presence of soaps and waxes as protective colloids, withwater. I

7. A process for the production of disperse s stems from hydrocarbonscontaining more t an 15 carbon atoms and water, consisting inemulsifying these hydrocarbons with aid of salts of unsymmetrlcaldiethylethylenediamine partially acylated with high molecular fattyacids containing 15 to 17 carbon atoms, in presence of soaps and Waxesas protective colloids, with water.

8. A process for the production of disperse systems from paraffin andwater, consistin 1n emulsifying paraflin with aid of the addition roductof benzyl chlorine and oleyl-diethy ethylenediamine, in presence ofsodium oleate and wax, with water.

9.9 1s new products the disperse systems consisting of water,lipoid-soluble s11)- stances, salts of partially acylated polyamines,and soaps and waxes as protective colloidsproducts the disperse systemsproducts'the disperse systems 13. As new products the disperse systems 1consisting of water,.lipoid -soluble substances, salts ofunsymmetrically alkylated diamines partially acylated with highmolecular fatty acids containing to 17 carbon atoms, and soaps and waxesas protective colloids.

14. As new products the disperse systems aemeer containing 15 to 17carbon atoms, and soaps and waxes as protective colloids.

16. As new products the disperse systems consisting of water,hydrocarbons containing more than 15 carbon atoms, the addition productof benzyl chloride and oleyl-diethylethylenediamine, soaps and waxes.

17. As new products the disperse systems I consisting of water,paraflin, .the addition product of benzyl chloride andoleyl-diethylethvlenediamine, sodium oleate and wax.

in witness whereof I have hereunto signed my name this 3rd day of March1931.

'55 NS KAGI.

